data_redmondite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'redmondite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H6 O20 Pb8 S8 Zn' _chemical_formula_weight 2305.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.1672(4) _cell_length_b 10.6576(4) _cell_length_c 14.0620(10) _cell_angle_alpha 90 _cell_angle_beta 101.173(7) _cell_angle_gamma 90 _cell_volume 1347.83(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7907 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'equant' _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 5.681 _exptl_crystal_F_000 1960 _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.090 _exptl_absorpt_coefficient_mu 51.337 _shelx_estimated_absorpt_T_min 0.071 _shelx_estimated_absorpt_T_max 0.091 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.415 _exptl_absorpt_process_details 'Higashi2001' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_number 9871 _diffrn_reflns_av_unetI/netI 0.0657 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.109 _diffrn_reflns_theta_max 25.026 _diffrn_reflns_theta_full 25.026 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 2372 _reflns_number_gt 2061 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+7.4268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_extinction_coef 0.00061(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2372 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.24391(6) 0.65742(5) 0.33075(4) 0.01579(18) Uani 1 1 d . . . . . Pb2 Pb 0.84077(6) 0.65986(5) 0.58783(4) 0.01615(18) Uani 1 1 d . . . . . Pb3 Pb 0.44282(6) 0.39015(5) 0.26232(4) 0.01803(18) Uani 1 1 d . . . . . Pb4 Pb 0.02065(6) 0.43840(5) 0.14031(4) 0.01675(18) Uani 1 1 d . . . . . Zn Zn 0.500000 0.500000 0.500000 0.0156(5) Uani 1 2 d S . P . . S1 S 0.8542(4) 0.6170(3) 0.3051(2) 0.0132(7) Uani 1 1 d . . . . . S2 S 0.2737(4) 0.8869(3) 0.5700(2) 0.0148(7) Uani 1 1 d . . . . . O1 O 0.7078(11) 0.6741(9) 0.2885(10) 0.037(3) Uani 1 1 d . . . . . O2 O 0.9264(12) 0.6429(9) 0.2229(8) 0.026(3) Uani 1 1 d . . . . . O3 O 0.9493(13) 0.6699(11) 0.3943(8) 0.040(3) Uani 1 1 d . . . . . S1A S 0.8353(4) 0.4313(4) 0.3181(3) 0.0248(9) Uani 1 1 d . . . . . O4 O 0.3125(13) 0.8178(10) 0.4898(9) 0.038(3) Uani 1 1 d . . . . . O5 O 0.1269(11) 0.8561(10) 0.5879(8) 0.027(3) Uani 1 1 d . . . . . O6 O 0.3861(12) 0.8684(9) 0.6615(8) 0.026(3) Uani 1 1 d . . . . . S2A S 0.2623(5) 0.0730(4) 0.5379(3) 0.0245(9) Uani 1 1 d . . . . . O7 O 0.2026(9) 0.4515(8) 0.2764(6) 0.0093(19) Uani 1 1 d . . . . . OH8 O 0.4840(10) 0.5746(8) 0.3643(6) 0.014(2) Uani 1 1 d . . . . . OH9 O 0.5784(10) 0.6664(9) 0.5790(7) 0.017(2) Uani 1 1 d . . . . . OH10 O 0.2641(9) 0.5364(8) 0.4700(7) 0.013(2) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0140(3) 0.0133(3) 0.0175(3) 0.0024(2) -0.0034(2) 0.0015(2) Pb2 0.0175(3) 0.0163(3) 0.0136(3) 0.0018(2) 0.0003(2) -0.0026(2) Pb3 0.0138(3) 0.0233(3) 0.0168(3) -0.0053(2) 0.0025(2) 0.0007(2) Pb4 0.0155(3) 0.0191(3) 0.0133(3) 0.0003(2) -0.0031(2) -0.0043(2) Zn 0.0158(12) 0.0194(13) 0.0089(12) 0.0022(10) -0.0043(9) 0.0010(9) S1 0.0107(18) 0.0135(18) 0.0155(19) 0.0000(14) 0.0025(14) -0.0006(13) S2 0.0170(19) 0.0140(18) 0.0111(18) -0.0023(14) -0.0030(14) 0.0037(14) O1 0.013(6) 0.015(6) 0.086(10) 0.007(6) 0.018(6) 0.010(4) O2 0.033(7) 0.023(6) 0.025(6) -0.003(5) 0.011(5) 0.002(5) O3 0.041(8) 0.047(8) 0.027(7) -0.012(6) -0.006(5) -0.011(6) S1A 0.026(2) 0.0163(19) 0.033(2) 0.0002(17) 0.0086(18) 0.0042(16) O4 0.042(8) 0.036(7) 0.033(7) -0.014(6) 0.004(6) 0.010(6) O5 0.022(6) 0.027(6) 0.033(7) 0.002(5) 0.005(5) 0.005(5) O6 0.030(6) 0.018(5) 0.024(6) -0.008(5) -0.010(5) 0.010(5) S2A 0.032(2) 0.019(2) 0.022(2) 0.0031(17) 0.0049(17) 0.0017(16) O7 0.007(5) 0.010(5) 0.010(5) -0.001(4) 0.001(4) 0.001(4) OH8 0.015(5) 0.014(5) 0.009(5) 0.004(4) -0.004(4) 0.005(4) OH9 0.015(5) 0.022(6) 0.012(5) 0.002(4) -0.003(4) 0.006(4) OH10 0.010(5) 0.007(5) 0.022(5) 0.004(4) 0.001(4) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 OH10 2.322(9) . ? Pb1 O7 2.330(8) . ? Pb1 OH8 2.333(9) . ? Pb1 O4 2.788(11) . ? Pb1 O6 2.940(11) 4_575 ? Pb1 O3 3.008(12) 1_455 ? Pb1 O2 3.015(11) 1_455 ? Pb1 O5 3.379(11) 4_575 ? Pb1 Zn 3.4388(6) . ? Pb1 S1 3.547(3) 1_455 ? Pb1 S1A 3.583(4) 2_655 ? Pb1 Pb3 3.6117(7) . ? Pb1 Pb2 3.7003(7) 3_666 ? Pb1 S2 3.759(4) 4_575 ? Pb1 Pb4 3.8320(8) . ? Pb2 O7 2.347(8) 3_666 ? Pb2 OH10 2.379(9) 3_666 ? Pb2 OH9 2.385(9) . ? Pb2 O2 2.839(10) 4_576 ? Pb2 O3 3.075(12) . ? Pb2 S1A 3.161(4) 3_766 ? Pb2 O5 3.355(10) 1_655 ? Pb2 S2A 3.388(4) 3_666 ? Pb2 Zn 3.5625(5) . ? Pb2 Pb3 3.6886(8) 3_666 ? Pb2 O1 3.730(11) 4_576 ? Pb2 S1 3.854(3) 4_576 ? Pb2 Pb4 3.9297(8) 3_666 ? Pb2 O3 3.991(12) 3_766 ? Pb3 O7 2.342(8) . ? Pb3 OH9 2.355(9) 3_666 ? Pb3 OH8 2.419(9) . ? Pb3 O1 2.708(9) 2_645 ? Pb3 O6 2.936(10) 4_575 ? Pb3 O6 3.247(10) 3_666 ? Pb3 S2A 3.290(4) 4_565 ? Pb3 Zn 3.4838(6) . ? Pb3 S1A 3.558(4) . ? Pb3 S2 3.707(3) 4_575 ? Pb3 O1 3.854(10) . ? Pb3 OH8 3.924(9) 2_645 ? Pb3 OH10 3.937(9) . ? Pb4 O7 2.286(9) . ? Pb4 O5 2.563(10) 4_575 ? Pb4 O2 2.690(10) 1_455 ? Pb4 S2A 2.869(4) 4_565 ? Pb4 O3 2.924(12) 2_645 ? Pb4 S2 3.274(3) 4_575 ? Pb4 S1A 3.285(4) 1_455 ? Pb4 O5 3.349(11) 2_545 ? Pb4 O4 3.487(12) 2_545 ? Pb4 S2A 3.543(4) 2 ? Pb4 S1 3.562(3) 1_455 ? Pb4 S2 3.638(4) 2_545 ? Pb4 S1 3.646(3) 2_645 ? Pb4 O2 3.673(10) 2_645 ? Pb4 O1 3.764(11) 2_645 ? Zn OH8 2.045(9) 3_666 ? Zn OH8 2.046(9) . ? Zn OH9 2.141(9) . ? Zn OH9 2.141(9) 3_666 ? Zn OH10 2.157(9) . ? Zn OH10 2.157(9) 3_666 ? S1 O1 1.451(10) . ? S1 O2 1.465(10) . ? S1 O3 1.493(11) . ? S1 S1A 1.999(5) . ? S2 O4 1.448(11) . ? S2 O5 1.454(11) . ? S2 O6 1.497(11) . ? S2 S2A 2.033(5) 1_565 ? O1 OH8 2.705(13) . ? O4 OH9 2.989(15) . ? O4 OH10 3.036(14) . ? O6 OH9 3.143(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag OH10 Pb1 O7 74.7(3) . . ? OH10 Pb1 OH8 72.6(3) . . ? O7 Pb1 OH8 78.3(3) . . ? OH10 Pb1 O4 72.3(3) . . ? O7 Pb1 O4 146.9(3) . . ? OH8 Pb1 O4 90.7(3) . . ? OH10 Pb1 O6 131.0(3) . 4_575 ? O7 Pb1 O6 73.5(3) . 4_575 ? OH8 Pb1 O6 65.1(3) . 4_575 ? O4 Pb1 O6 129.8(3) . 4_575 ? OH10 Pb1 O3 72.7(3) . 1_455 ? O7 Pb1 O3 92.4(3) . 1_455 ? OH8 Pb1 O3 145.4(3) . 1_455 ? O4 Pb1 O3 79.1(3) . 1_455 ? O6 Pb1 O3 144.0(3) 4_575 1_455 ? OH10 Pb1 O2 107.9(3) . 1_455 ? O7 Pb1 O2 73.0(3) . 1_455 ? OH8 Pb1 O2 149.7(3) . 1_455 ? O4 Pb1 O2 118.7(3) . 1_455 ? O6 Pb1 O2 97.1(3) 4_575 1_455 ? O3 Pb1 O2 46.9(3) 1_455 1_455 ? OH10 Pb1 O5 141.9(3) . 4_575 ? O7 Pb1 O5 68.2(3) . 4_575 ? OH8 Pb1 O5 106.9(3) . 4_575 ? O4 Pb1 O5 144.6(3) . 4_575 ? O6 Pb1 O5 44.1(3) 4_575 4_575 ? O3 Pb1 O5 100.1(3) 1_455 4_575 ? O2 Pb1 O5 53.3(3) 1_455 4_575 ? OH10 Pb1 Zn 38.1(2) . . ? O7 Pb1 Zn 79.3(2) . . ? OH8 Pb1 Zn 35.4(2) . . ? O4 Pb1 Zn 74.1(2) . . ? O6 Pb1 Zn 99.5(2) 4_575 . ? O3 Pb1 Zn 110.4(2) 1_455 . ? O2 Pb1 Zn 141.85(19) 1_455 . ? O5 Pb1 Zn 135.99(18) 4_575 . ? OH10 Pb1 S1 86.1(2) . 1_455 ? O7 Pb1 S1 75.9(2) . 1_455 ? OH8 Pb1 S1 150.1(2) . 1_455 ? O4 Pb1 S1 102.8(2) . 1_455 ? O6 Pb1 S1 120.1(2) 4_575 1_455 ? O3 Pb1 S1 24.6(2) 1_455 1_455 ? O2 Pb1 S1 24.1(2) 1_455 1_455 ? O5 Pb1 S1 77.04(18) 4_575 1_455 ? Zn Pb1 S1 123.40(6) . 1_455 ? OH10 Pb1 S1A 156.8(2) . 2_655 ? O7 Pb1 S1A 125.0(2) . 2_655 ? OH8 Pb1 S1A 120.2(2) . 2_655 ? O4 Pb1 S1A 87.6(3) . 2_655 ? O6 Pb1 S1A 71.0(2) 4_575 2_655 ? O3 Pb1 S1A 92.6(2) 1_455 2_655 ? O2 Pb1 S1A 71.4(2) 1_455 2_655 ? O5 Pb1 S1A 57.01(19) 4_575 2_655 ? Zn Pb1 S1A 146.68(7) . 2_655 ? S1 Pb1 S1A 87.32(8) 1_455 2_655 ? OH10 Pb1 Pb3 79.9(2) . . ? O7 Pb1 Pb3 39.5(2) . . ? OH8 Pb1 Pb3 41.4(2) . . ? O4 Pb1 Pb3 130.6(2) . . ? O6 Pb1 Pb3 52.0(2) 4_575 . ? O3 Pb1 Pb3 130.0(2) 1_455 . ? O2 Pb1 Pb3 108.29(19) 1_455 . ? O5 Pb1 Pb3 76.99(18) 4_575 . ? Zn Pb1 Pb3 59.163(12) . . ? S1 Pb1 Pb3 115.33(6) 1_455 . ? S1A Pb1 Pb3 122.84(7) 2_655 . ? OH10 Pb1 Pb2 38.6(2) . 3_666 ? O7 Pb1 Pb2 37.9(2) . 3_666 ? OH8 Pb1 Pb2 80.7(2) . 3_666 ? O4 Pb1 Pb2 109.9(3) . 3_666 ? O6 Pb1 Pb2 108.52(19) 4_575 3_666 ? O3 Pb1 Pb2 72.2(2) 1_455 3_666 ? O2 Pb1 Pb2 82.46(19) 1_455 3_666 ? O5 Pb1 Pb2 103.26(17) 4_575 3_666 ? Zn Pb1 Pb2 59.736(12) . 3_666 ? S1 Pb1 Pb2 69.70(6) 1_455 3_666 ? S1A Pb1 Pb2 153.41(7) 2_655 3_666 ? Pb3 Pb1 Pb2 60.575(15) . 3_666 ? OH10 Pb1 S2 138.1(2) . 4_575 ? O7 Pb1 S2 66.4(2) . 4_575 ? OH8 Pb1 S2 84.6(2) . 4_575 ? O4 Pb1 S2 144.3(3) . 4_575 ? O6 Pb1 S2 21.7(2) 4_575 4_575 ? O3 Pb1 S2 122.3(2) 1_455 4_575 ? O2 Pb1 S2 75.43(19) 1_455 4_575 ? O5 Pb1 S2 22.71(18) 4_575 4_575 ? Zn Pb1 S2 116.42(6) . 4_575 ? S1 Pb1 S2 98.49(8) 1_455 4_575 ? S1A Pb1 S2 64.99(8) 2_655 4_575 ? Pb3 Pb1 S2 60.34(5) . 4_575 ? Pb2 Pb1 S2 104.26(5) 3_666 4_575 ? OH10 Pb1 Pb4 101.3(2) . . ? O7 Pb1 Pb4 33.5(2) . . ? OH8 Pb1 Pb4 105.4(2) . . ? O4 Pb1 Pb4 160.2(2) . . ? O6 Pb1 Pb4 68.77(19) 4_575 . ? O3 Pb1 Pb4 81.1(2) 1_455 . ? O2 Pb1 Pb4 44.30(18) 1_455 . ? O5 Pb1 Pb4 41.04(17) 4_575 . ? Zn Pb1 Pb4 112.770(16) . . ? S1 Pb1 Pb4 57.58(6) 1_455 . ? S1A Pb1 Pb4 93.88(7) 2_655 . ? Pb3 Pb1 Pb4 64.041(15) . . ? Pb2 Pb1 Pb4 62.866(15) 3_666 . ? S2 Pb1 Pb4 51.09(5) 4_575 . ? O7 Pb2 OH10 73.3(3) 3_666 3_666 ? O7 Pb2 OH9 74.3(3) 3_666 . ? OH10 Pb2 OH9 70.8(3) 3_666 . ? O7 Pb2 O2 84.2(3) 3_666 4_576 ? OH10 Pb2 O2 157.0(3) 3_666 4_576 ? OH9 Pb2 O2 99.1(3) . 4_576 ? O7 Pb2 O3 150.8(3) 3_666 . ? OH10 Pb2 O3 84.6(3) 3_666 . ? OH9 Pb2 O3 116.7(3) . . ? O2 Pb2 O3 118.1(3) 4_576 . ? O7 Pb2 S1A 78.3(2) 3_666 3_766 ? OH10 Pb2 S1A 99.1(2) 3_666 3_766 ? OH9 Pb2 S1A 152.5(2) . 3_766 ? O2 Pb2 S1A 80.3(2) 4_576 3_766 ? O3 Pb2 S1A 86.7(2) . 3_766 ? O7 Pb2 O5 124.8(3) 3_666 1_655 ? OH10 Pb2 O5 144.3(3) 3_666 1_655 ? OH9 Pb2 O5 139.7(3) . 1_655 ? O2 Pb2 O5 54.8(3) 4_576 1_655 ? O3 Pb2 O5 65.9(3) . 1_655 ? S1A Pb2 O5 61.33(19) 3_766 1_655 ? O7 Pb2 S2A 140.9(2) 3_666 3_666 ? OH10 Pb2 S2A 120.5(2) 3_666 3_666 ? OH9 Pb2 S2A 76.8(2) . 3_666 ? O2 Pb2 S2A 74.9(2) 4_576 3_666 ? O3 Pb2 S2A 67.3(2) . 3_666 ? S1A Pb2 S2A 128.40(10) 3_766 3_666 ? O5 Pb2 S2A 67.37(19) 1_655 3_666 ? O7 Pb2 Zn 76.4(2) 3_666 . ? OH10 Pb2 Zn 36.1(2) 3_666 . ? OH9 Pb2 Zn 35.7(2) . . ? O2 Pb2 Zn 134.1(2) 4_576 . ? O3 Pb2 Zn 97.0(2) . . ? S1A Pb2 Zn 133.45(7) 3_766 . ? O5 Pb2 Zn 158.64(18) 1_655 . ? S2A Pb2 Zn 94.80(7) 3_666 . ? O7 Pb2 Pb3 38.1(2) 3_666 3_666 ? OH10 Pb2 Pb3 77.6(2) 3_666 3_666 ? OH9 Pb2 Pb3 38.6(2) . 3_666 ? O2 Pb2 Pb3 81.9(2) 4_576 3_666 ? O3 Pb2 Pb3 153.5(2) . 3_666 ? S1A Pb2 Pb3 115.19(7) 3_766 3_666 ? O5 Pb2 Pb3 136.69(18) 1_655 3_666 ? S2A Pb2 Pb3 105.27(7) 3_666 3_666 ? Zn Pb2 Pb3 57.398(12) . 3_666 ? O7 Pb2 Pb1 37.6(2) 3_666 3_666 ? OH10 Pb2 Pb1 37.5(2) 3_666 3_666 ? OH9 Pb2 Pb1 76.9(2) . 3_666 ? O2 Pb2 Pb1 121.1(2) 4_576 3_666 ? O3 Pb2 Pb1 115.4(2) . 3_666 ? S1A Pb2 Pb1 79.98(7) 3_766 3_666 ? O5 Pb2 Pb1 141.31(18) 1_655 3_666 ? S2A Pb2 Pb1 151.09(7) 3_666 3_666 ? Zn Pb2 Pb1 56.482(12) . 3_666 ? Pb3 Pb2 Pb1 58.523(14) 3_666 3_666 ? O7 Pb2 O1 59.5(3) 3_666 4_576 ? OH10 Pb2 O1 120.4(3) 3_666 4_576 ? OH9 Pb2 O1 63.4(3) . 4_576 ? O2 Pb2 O1 39.8(2) 4_576 4_576 ? O3 Pb2 O1 149.6(3) . 4_576 ? S1A Pb2 O1 104.3(2) 3_766 4_576 ? O5 Pb2 O1 94.3(2) 1_655 4_576 ? S2A Pb2 O1 84.11(19) 3_666 4_576 ? Zn Pb2 O1 95.51(16) . 4_576 ? Pb3 Pb2 O1 42.82(14) 3_666 4_576 ? Pb1 Pb2 O1 94.61(15) 3_666 4_576 ? O7 Pb2 S1 69.6(2) 3_666 4_576 ? OH10 Pb2 S1 139.7(2) 3_666 4_576 ? OH9 Pb2 S1 84.3(2) . 4_576 ? O2 Pb2 S1 18.4(2) 4_576 4_576 ? O3 Pb2 S1 135.5(2) . 4_576 ? S1A Pb2 S1 88.56(9) 3_766 4_576 ? O5 Pb2 S1 73.16(19) 1_655 4_576 ? S2A Pb2 S1 81.85(9) 3_666 4_576 ? Zn Pb2 S1 117.45(5) . 4_576 ? Pb3 Pb2 S1 63.52(5) 3_666 4_576 ? Pb1 Pb2 S1 107.15(5) 3_666 4_576 ? O1 Pb2 S1 21.98(16) 4_576 4_576 ? O7 Pb2 Pb4 31.5(2) 3_666 3_666 ? OH10 Pb2 Pb4 97.5(2) 3_666 3_666 ? OH9 Pb2 Pb4 101.0(2) . 3_666 ? O2 Pb2 Pb4 63.3(2) 4_576 3_666 ? O3 Pb2 Pb4 140.5(2) . 3_666 ? S1A Pb2 Pb4 53.89(7) 3_766 3_666 ? O5 Pb2 Pb4 93.47(18) 1_655 3_666 ? S2A Pb2 Pb4 137.45(7) 3_666 3_666 ? Zn Pb2 Pb4 107.835(16) . 3_666 ? Pb3 Pb2 Pb4 62.390(15) 3_666 3_666 ? Pb1 Pb2 Pb4 60.207(14) 3_666 3_666 ? O1 Pb2 Pb4 58.79(19) 4_576 3_666 ? S1 Pb2 Pb4 55.86(5) 4_576 3_666 ? O7 Pb2 O3 70.1(3) 3_666 3_766 ? OH10 Pb2 O3 53.5(3) 3_666 3_766 ? OH9 Pb2 O3 119.9(3) . 3_766 ? O2 Pb2 O3 122.8(3) 4_576 3_766 ? O3 Pb2 O3 81.5(3) . 3_766 ? S1A Pb2 O3 45.62(17) 3_766 3_766 ? O5 Pb2 O3 100.5(2) 1_655 3_766 ? S2A Pb2 O3 148.77(18) 3_666 3_766 ? Zn Pb2 O3 88.87(16) . 3_766 ? Pb3 Pb2 O3 102.79(18) 3_666 3_766 ? Pb1 Pb2 O3 45.84(17) 3_666 3_766 ? O1 Pb2 O3 126.5(3) 4_576 3_766 ? S1 Pb2 O3 123.53(17) 4_576 3_766 ? Pb4 Pb2 O3 69.09(17) 3_666 3_766 ? O7 Pb3 OH9 74.9(3) . 3_666 ? O7 Pb3 OH8 76.4(3) . . ? OH9 Pb3 OH8 71.2(3) 3_666 . ? O7 Pb3 O1 79.6(3) . 2_645 ? OH9 Pb3 O1 84.3(4) 3_666 2_645 ? OH8 Pb3 O1 149.3(3) . 2_645 ? O7 Pb3 O6 73.4(3) . 4_575 ? OH9 Pb3 O6 130.0(3) 3_666 4_575 ? OH8 Pb3 O6 64.3(3) . 4_575 ? O1 Pb3 O6 125.7(3) 2_645 4_575 ? O7 Pb3 O6 127.7(3) . 3_666 ? OH9 Pb3 O6 66.0(3) 3_666 3_666 ? OH8 Pb3 O6 118.9(3) . 3_666 ? O1 Pb3 O6 63.6(3) 2_645 3_666 ? O6 Pb3 O6 158.75(5) 4_575 3_666 ? O7 Pb3 S2A 75.0(2) . 4_565 ? OH9 Pb3 S2A 145.1(2) 3_666 4_565 ? OH8 Pb3 S2A 117.6(2) . 4_565 ? O1 Pb3 S2A 73.3(3) 2_645 4_565 ? O6 Pb3 S2A 54.8(2) 4_575 4_565 ? O6 Pb3 S2A 122.59(19) 3_666 4_565 ? O7 Pb3 Zn 78.1(2) . . ? OH9 Pb3 Zn 37.0(2) 3_666 . ? OH8 Pb3 Zn 35.0(2) . . ? O1 Pb3 Zn 120.9(3) 2_645 . ? O6 Pb3 Zn 98.5(2) 4_575 . ? O6 Pb3 Zn 89.73(18) 3_666 . ? S2A Pb3 Zn 146.53(7) 4_565 . ? O7 Pb3 S1A 150.9(2) . . ? OH9 Pb3 S1A 95.1(2) 3_666 . ? OH8 Pb3 S1A 74.6(2) . . ? O1 Pb3 S1A 127.2(2) 2_645 . ? O6 Pb3 S1A 94.3(2) 4_575 . ? O6 Pb3 S1A 68.2(2) 3_666 . ? S2A Pb3 S1A 119.73(10) 4_565 . ? Zn Pb3 S1A 77.83(7) . . ? O7 Pb3 Pb1 39.3(2) . . ? OH9 Pb3 Pb1 79.1(2) 3_666 . ? OH8 Pb3 Pb1 39.7(2) . . ? O1 Pb3 Pb1 118.9(2) 2_645 . ? O6 Pb3 Pb1 52.1(2) 4_575 . ? O6 Pb3 Pb1 144.85(19) 3_666 . ? S2A Pb3 Pb1 88.59(7) 4_565 . ? Zn Pb3 Pb1 57.945(12) . . ? S1A Pb3 Pb1 112.66(6) . . ? O7 Pb3 Pb2 38.2(2) . 3_666 ? OH9 Pb3 Pb2 39.2(2) 3_666 3_666 ? OH8 Pb3 Pb2 79.9(2) . 3_666 ? O1 Pb3 Pb2 69.4(2) 2_645 3_666 ? O6 Pb3 Pb2 108.9(2) 4_575 3_666 ? O6 Pb3 Pb2 92.2(2) 3_666 3_666 ? S2A Pb3 Pb2 106.62(7) 4_565 3_666 ? Zn Pb3 Pb2 59.483(13) . 3_666 ? S1A Pb3 Pb2 133.34(7) . 3_666 ? Pb1 Pb3 Pb2 60.901(15) . 3_666 ? O7 Pb3 S2 67.4(2) . 4_575 ? OH9 Pb3 S2 139.1(2) 3_666 4_575 ? OH8 Pb3 S2 84.7(2) . 4_575 ? O1 Pb3 S2 103.4(3) 2_645 4_575 ? O6 Pb3 S2 22.4(2) 4_575 4_575 ? O6 Pb3 S2 153.07(19) 3_666 4_575 ? S2A Pb3 S2 33.10(8) 4_565 4_575 ? Zn Pb3 S2 116.65(6) . 4_575 ? S1A Pb3 S2 110.12(9) . 4_575 ? Pb1 Pb3 S2 61.80(6) . 4_575 ? Pb2 Pb3 S2 105.55(6) 3_666 4_575 ? O7 Pb3 O1 111.0(2) . . ? OH9 Pb3 O1 106.0(3) 3_666 . ? OH8 Pb3 O1 44.1(3) . . ? O1 Pb3 O1 166.54(12) 2_645 . ? O6 Pb3 O1 53.6(3) 4_575 . ? O6 Pb3 O1 112.3(2) 3_666 . ? S2A Pb3 O1 100.9(2) 4_565 . ? Zn Pb3 O1 70.69(19) . . ? S1A Pb3 O1 44.79(15) . . ? Pb1 Pb3 O1 72.33(14) . . ? Pb2 Pb3 O1 124.04(17) 3_666 . ? S2 Pb3 O1 74.51(19) 4_575 . ? O7 Pb3 OH8 121.6(2) . 2_645 ? OH9 Pb3 OH8 105.3(3) 3_666 2_645 ? OH8 Pb3 OH8 160.85(10) . 2_645 ? O1 Pb3 OH8 43.5(2) 2_645 2_645 ? O6 Pb3 OH8 124.2(3) 4_575 2_645 ? O6 Pb3 OH8 46.3(2) 3_666 2_645 ? S2A Pb3 OH8 76.43(15) 4_565 2_645 ? Zn Pb3 OH8 135.75(13) . 2_645 ? S1A Pb3 OH8 87.21(14) . 2_645 ? Pb1 Pb3 OH8 159.47(13) . 2_645 ? Pb2 Pb3 OH8 109.68(13) 3_666 2_645 ? S2 Pb3 OH8 107.60(14) 4_575 2_645 ? O1 Pb3 OH8 123.8(2) . 2_645 ? O7 Pb3 OH10 45.1(2) . . ? OH9 Pb3 OH10 43.6(3) 3_666 . ? OH8 Pb3 OH10 43.8(2) . . ? O1 Pb3 OH10 105.6(3) 2_645 . ? O6 Pb3 OH10 87.2(2) 4_575 . ? O6 Pb3 OH10 109.6(2) 3_666 . ? S2A Pb3 OH10 117.39(15) 4_565 . ? Zn Pb3 OH10 33.08(13) . . ? S1A Pb3 OH10 109.63(14) . . ? Pb1 Pb3 OH10 35.50(13) . . ? Pb2 Pb3 OH10 36.17(12) 3_666 . ? S2 Pb3 OH10 96.44(14) 4_575 . ? O1 Pb3 OH10 87.9(2) . . ? OH8 Pb3 OH10 143.95(18) 2_645 . ? O7 Pb4 O5 86.1(3) . 4_575 ? O7 Pb4 O2 80.4(3) . 1_455 ? O5 Pb4 O2 66.6(3) 4_575 1_455 ? O7 Pb4 S2A 85.0(2) . 4_565 ? O5 Pb4 S2A 61.2(2) 4_575 4_565 ? O2 Pb4 S2A 126.5(2) 1_455 4_565 ? O7 Pb4 O3 97.0(3) . 2_645 ? O5 Pb4 O3 137.3(3) 4_575 2_645 ? O2 Pb4 O3 156.0(3) 1_455 2_645 ? S2A Pb4 O3 76.6(3) 4_565 2_645 ? O7 Pb4 S2 76.9(2) . 4_575 ? O5 Pb4 S2 25.3(2) 4_575 4_575 ? O2 Pb4 S2 88.6(2) 1_455 4_575 ? S2A Pb4 S2 37.93(10) 4_565 4_575 ? O3 Pb4 S2 114.3(3) 2_645 4_575 ? O7 Pb4 S1A 76.4(2) . 1_455 ? O5 Pb4 S1A 121.3(2) 4_575 1_455 ? O2 Pb4 S1A 55.5(2) 1_455 1_455 ? S2A Pb4 S1A 160.83(12) 4_565 1_455 ? O3 Pb4 S1A 100.6(2) 2_645 1_455 ? S2 Pb4 S1A 138.11(9) 4_575 1_455 ? O7 Pb4 O5 155.8(3) . 2_545 ? O5 Pb4 O5 93.1(3) 4_575 2_545 ? O2 Pb4 O5 121.5(3) 1_455 2_545 ? S2A Pb4 O5 73.50(19) 4_565 2_545 ? O3 Pb4 O5 67.5(3) 2_645 2_545 ? S2 Pb4 O5 92.17(18) 4_575 2_545 ? S1A Pb4 O5 123.42(19) 1_455 2_545 ? O7 Pb4 O4 152.2(3) . 2_545 ? O5 Pb4 O4 120.5(3) 4_575 2_545 ? O2 Pb4 O4 101.7(3) 1_455 2_545 ? S2A Pb4 O4 113.8(2) 4_565 2_545 ? O3 Pb4 O4 69.7(3) 2_645 2_545 ? S2 Pb4 O4 130.62(19) 4_575 2_545 ? S1A Pb4 O4 82.0(2) 1_455 2_545 ? O5 Pb4 O4 41.5(3) 2_545 2_545 ? O7 Pb4 S2A 152.0(2) . 2 ? O5 Pb4 S2A 73.6(2) 4_575 2 ? O2 Pb4 S2A 74.0(2) 1_455 2 ? S2A Pb4 S2A 101.12(10) 4_565 2 ? O3 Pb4 S2A 111.0(2) 2_645 2 ? S2 Pb4 S2A 91.18(9) 4_575 2 ? S1A Pb4 S2A 97.58(10) 1_455 2 ? O5 Pb4 S2A 47.44(19) 2_545 2 ? O4 Pb4 S2A 48.03(19) 2_545 2 ? O7 Pb4 S1 76.0(2) . 1_455 ? O5 Pb4 S1 88.0(2) 4_575 1_455 ? O2 Pb4 S1 21.9(2) 1_455 1_455 ? S2A Pb4 S1 144.95(9) 4_565 1_455 ? O3 Pb4 S1 134.2(2) 2_645 1_455 ? S2 Pb4 S1 108.08(8) 4_575 1_455 ? S1A Pb4 S1 33.63(8) 1_455 1_455 ? O5 Pb4 S1 128.23(19) 2_545 1_455 ? O4 Pb4 S1 95.5(2) 2_545 1_455 ? S2A Pb4 S1 84.06(9) 2 1_455 ? O7 Pb4 S2 174.6(2) . 2_545 ? O5 Pb4 S2 99.1(2) 4_575 2_545 ? O2 Pb4 S2 102.9(2) 1_455 2_545 ? S2A Pb4 S2 96.26(10) 4_565 2_545 ? O3 Pb4 S2 78.2(2) 2_645 2_545 ? S2 Pb4 S2 107.33(7) 4_575 2_545 ? S1A Pb4 S2 101.75(9) 1_455 2_545 ? O5 Pb4 S2 23.55(18) 2_545 2_545 ? O4 Pb4 S2 23.32(18) 2_545 2_545 ? S2A Pb4 S2 32.85(8) 2 2_545 ? S1 Pb4 S2 105.40(8) 1_455 2_545 ? O7 Pb4 S1 74.5(2) . 2_645 ? O5 Pb4 S1 137.9(2) 4_575 2_645 ? O2 Pb4 S1 141.7(2) 1_455 2_645 ? S2A Pb4 S1 79.85(9) 4_565 2_645 ? O3 Pb4 S1 23.1(2) 2_645 2_645 ? S2 Pb4 S1 112.67(8) 4_575 2_645 ? S1A Pb4 S1 90.35(8) 1_455 2_645 ? O5 Pb4 S1 90.46(19) 2_545 2_645 ? O4 Pb4 S1 88.41(19) 2_545 2_645 ? S2A Pb4 S1 133.38(8) 2 2_645 ? S1 Pb4 S1 121.46(5) 1_455 2_645 ? S2 Pb4 S1 100.54(8) 2_545 2_645 ? O7 Pb4 O2 67.2(3) . 2_645 ? O5 Pb4 O2 149.8(3) 4_575 2_645 ? O2 Pb4 O2 119.32(8) 1_455 2_645 ? S2A Pb4 O2 100.94(17) 4_565 2_645 ? O3 Pb4 O2 40.6(3) 2_645 2_645 ? S2 Pb4 O2 128.05(18) 4_575 2_645 ? S1A Pb4 O2 67.48(17) 1_455 2_645 ? O5 Pb4 O2 105.4(2) 2_545 2_645 ? O4 Pb4 O2 88.4(2) 2_545 2_645 ? S2A Pb4 O2 136.23(18) 2 2_645 ? S1 Pb4 O2 98.48(17) 1_455 2_645 ? S2 Pb4 O2 107.35(18) 2_545 2_645 ? S1 Pb4 O2 23.08(16) 2_645 2_645 ? O7 Pb4 O1 59.0(3) . 2_645 ? O5 Pb4 O1 116.6(3) 4_575 2_645 ? O2 Pb4 O1 138.0(3) 1_455 2_645 ? S2A Pb4 O1 64.30(19) 4_565 2_645 ? O3 Pb4 O1 39.9(3) 2_645 2_645 ? S2 Pb4 O1 92.00(16) 4_575 2_645 ? S1A Pb4 O1 101.16(19) 1_455 2_645 ? O5 Pb4 O1 100.5(3) 2_545 2_645 ? O4 Pb4 O1 109.3(2) 2_545 2_645 ? S2A Pb4 O1 147.9(2) 2 2_645 ? S1 Pb4 O1 124.9(2) 1_455 2_645 ? S2 Pb4 O1 116.83(19) 2_545 2_645 ? S1 Pb4 O1 22.51(15) 2_645 2_645 ? O2 Pb4 O1 37.4(2) 2_645 2_645 ? OH8 Zn OH8 180.0 3_666 . ? OH8 Zn OH9 83.2(4) 3_666 . ? OH8 Zn OH9 96.8(4) . . ? OH8 Zn OH9 96.8(4) 3_666 3_666 ? OH8 Zn OH9 83.2(4) . 3_666 ? OH9 Zn OH9 180.0(5) . 3_666 ? OH8 Zn OH10 98.1(3) 3_666 . ? OH8 Zn OH10 81.9(3) . . ? OH9 Zn OH10 100.1(3) . . ? OH9 Zn OH10 79.9(3) 3_666 . ? OH8 Zn OH10 81.9(3) 3_666 3_666 ? OH8 Zn OH10 98.1(3) . 3_666 ? OH9 Zn OH10 79.9(3) . 3_666 ? OH9 Zn OH10 100.1(3) 3_666 3_666 ? OH10 Zn OH10 180.0 . 3_666 ? OH8 Zn Pb1 41.3(2) 3_666 3_666 ? OH8 Zn Pb1 138.7(2) . 3_666 ? OH9 Zn Pb1 86.0(2) . 3_666 ? OH9 Zn Pb1 94.0(2) 3_666 3_666 ? OH10 Zn Pb1 138.4(2) . 3_666 ? OH10 Zn Pb1 41.6(2) 3_666 3_666 ? OH8 Zn Pb1 138.7(2) 3_666 . ? OH8 Zn Pb1 41.3(2) . . ? OH9 Zn Pb1 94.0(2) . . ? OH9 Zn Pb1 86.0(2) 3_666 . ? OH10 Zn Pb1 41.6(2) . . ? OH10 Zn Pb1 138.4(2) 3_666 . ? Pb1 Zn Pb1 180.0 3_666 . ? OH8 Zn Pb3 42.7(3) 3_666 3_666 ? OH8 Zn Pb3 137.3(3) . 3_666 ? OH9 Zn Pb3 41.5(2) . 3_666 ? OH9 Zn Pb3 138.5(2) 3_666 3_666 ? OH10 Zn Pb3 94.9(2) . 3_666 ? OH10 Zn Pb3 85.1(2) 3_666 3_666 ? Pb1 Zn Pb3 62.892(13) 3_666 3_666 ? Pb1 Zn Pb3 117.108(13) . 3_666 ? OH8 Zn Pb3 137.3(3) 3_666 . ? OH8 Zn Pb3 42.7(3) . . ? OH9 Zn Pb3 138.5(2) . . ? OH9 Zn Pb3 41.5(2) 3_666 . ? OH10 Zn Pb3 85.1(2) . . ? OH10 Zn Pb3 94.9(2) 3_666 . ? Pb1 Zn Pb3 117.108(13) 3_666 . ? Pb1 Zn Pb3 62.892(13) . . ? Pb3 Zn Pb3 180.0 3_666 . ? OH8 Zn Pb2 87.9(3) 3_666 . ? OH8 Zn Pb2 92.1(3) . . ? OH9 Zn Pb2 40.6(2) . . ? OH9 Zn Pb2 139.4(2) 3_666 . ? OH10 Zn Pb2 139.5(2) . . ? OH10 Zn Pb2 40.5(2) 3_666 . ? Pb1 Zn Pb2 63.781(13) 3_666 . ? Pb1 Zn Pb2 116.219(13) . . ? Pb3 Zn Pb2 63.120(13) 3_666 . ? Pb3 Zn Pb2 116.881(13) . . ? OH8 Zn Pb2 92.1(3) 3_666 3_666 ? OH8 Zn Pb2 87.9(3) . 3_666 ? OH9 Zn Pb2 139.4(2) . 3_666 ? OH9 Zn Pb2 40.6(2) 3_666 3_666 ? OH10 Zn Pb2 40.5(2) . 3_666 ? OH10 Zn Pb2 139.5(2) 3_666 3_666 ? Pb1 Zn Pb2 116.218(13) 3_666 3_666 ? Pb1 Zn Pb2 63.782(13) . 3_666 ? Pb3 Zn Pb2 116.880(13) 3_666 3_666 ? Pb3 Zn Pb2 63.119(13) . 3_666 ? Pb2 Zn Pb2 180.0 . 3_666 ? O1 S1 O2 109.9(7) . . ? O1 S1 O3 110.4(7) . . ? O2 S1 O3 108.2(7) . . ? O1 S1 S1A 109.6(4) . . ? O2 S1 S1A 108.6(4) . . ? O3 S1 S1A 110.1(5) . . ? O1 S1 Pb1 148.0(4) . 1_655 ? O2 S1 Pb1 57.1(5) . 1_655 ? O3 S1 Pb1 57.0(5) . 1_655 ? S1A S1 Pb1 102.38(17) . 1_655 ? O1 S1 Pb4 128.3(5) . 1_655 ? O2 S1 Pb4 43.3(4) . 1_655 ? O3 S1 Pb4 119.6(5) . 1_655 ? S1A S1 Pb4 65.56(14) . 1_655 ? Pb1 S1 Pb4 65.24(6) 1_655 1_655 ? O1 S1 Pb4 83.3(4) . 2_655 ? O2 S1 Pb4 79.5(4) . 2_655 ? O3 S1 Pb4 50.2(5) . 2_655 ? S1A S1 Pb4 160.1(2) . 2_655 ? Pb1 S1 Pb4 66.11(6) 1_655 2_655 ? Pb4 S1 Pb4 118.82(9) 1_655 2_655 ? O1 S1 Pb2 74.2(5) . 4_575 ? O2 S1 Pb2 37.7(4) . 4_575 ? O3 S1 Pb2 110.9(5) . 4_575 ? S1A S1 Pb2 133.94(19) . 4_575 ? Pb1 S1 Pb2 83.27(7) 1_655 4_575 ? Pb4 S1 Pb2 76.48(7) 1_655 4_575 ? Pb4 S1 Pb2 63.12(5) 2_655 4_575 ? O1 S1 Pb3 23.7(4) . 2_655 ? O2 S1 Pb3 93.9(4) . 2_655 ? O3 S1 Pb3 100.7(5) . 2_655 ? S1A S1 Pb3 132.83(18) . 2_655 ? Pb1 S1 Pb3 124.45(9) 1_655 2_655 ? Pb4 S1 Pb3 126.63(10) 1_655 2_655 ? Pb4 S1 Pb3 62.30(5) 2_655 2_655 ? Pb2 S1 Pb3 56.21(5) 4_575 2_655 ? O1 S1 Pb2 84.6(5) . . ? O2 S1 Pb2 149.6(5) . . ? O3 S1 Pb2 41.6(5) . . ? S1A S1 Pb2 90.09(16) . . ? Pb1 S1 Pb2 96.23(8) 1_655 . ? Pb4 S1 Pb2 143.27(10) 1_655 . ? Pb4 S1 Pb2 75.77(6) 2_655 . ? Pb2 S1 Pb2 135.25(9) 4_575 . ? Pb3 S1 Pb2 90.10(7) 2_655 . ? O1 S1 Pb2 153.5(4) . 3_766 ? O2 S1 Pb2 92.6(4) . 3_766 ? O3 S1 Pb2 73.7(5) . 3_766 ? S1A S1 Pb2 47.59(14) . 3_766 ? Pb1 S1 Pb2 56.89(5) 1_655 3_766 ? Pb4 S1 Pb2 60.77(5) 1_655 3_766 ? Pb4 S1 Pb2 115.46(9) 2_655 3_766 ? Pb2 S1 Pb2 130.03(8) 4_575 3_766 ? Pb3 S1 Pb2 172.60(10) 2_655 3_766 ? Pb2 S1 Pb2 82.50(7) . 3_766 ? O1 S1 Pb3 58.0(4) . . ? O2 S1 Pb3 120.0(5) . . ? O3 S1 Pb3 131.6(5) . . ? S1A S1 Pb3 51.97(14) . . ? Pb1 S1 Pb3 153.63(9) 1_655 . ? Pb4 S1 Pb3 94.64(7) 1_655 . ? Pb4 S1 Pb3 140.14(9) 2_655 . ? Pb2 S1 Pb3 109.52(8) 4_575 . ? Pb3 S1 Pb3 80.86(6) 2_655 . ? Pb2 S1 Pb3 90.44(6) . . ? Pb2 S1 Pb3 99.07(7) 3_766 . ? O4 S2 O5 113.3(7) . . ? O4 S2 O6 111.7(7) . . ? O5 S2 O6 109.1(6) . . ? O4 S2 S2A 109.5(5) . 1_565 ? O5 S2 S2A 104.4(4) . 1_565 ? O6 S2 S2A 108.4(5) . 1_565 ? O4 S2 Pb4 145.1(5) . 4_576 ? O5 S2 Pb4 48.9(4) . 4_576 ? O6 S2 Pb4 103.0(4) . 4_576 ? S2A S2 Pb4 60.19(14) 1_565 4_576 ? O4 S2 Pb4 72.5(5) . 2 ? O5 S2 Pb4 67.0(4) . 2 ? O6 S2 Pb4 175.4(5) . 2 ? S2A S2 Pb4 70.99(15) 1_565 2 ? Pb4 S2 Pb4 72.67(7) 4_576 2 ? O4 S2 Pb3 139.8(5) . 4_576 ? O5 S2 Pb3 106.8(4) . 4_576 ? O6 S2 Pb3 48.4(4) . 4_576 ? S2A S2 Pb3 62.12(14) 1_565 4_576 ? Pb4 S2 Pb3 68.63(6) 4_576 4_576 ? Pb4 S2 Pb3 129.47(9) 2 4_576 ? O4 S2 Pb1 140.5(5) . 4_576 ? O5 S2 Pb1 63.8(4) . 4_576 ? O6 S2 Pb1 46.6(4) . 4_576 ? S2A S2 Pb1 109.18(16) 1_565 4_576 ? Pb4 S2 Pb1 65.61(6) 4_576 4_576 ? Pb4 S2 Pb1 128.98(10) 2 4_576 ? Pb3 S2 Pb1 57.86(5) 4_576 4_576 ? O4 S2 Pb1 18.3(5) . . ? O5 S2 Pb1 95.2(4) . . ? O6 S2 Pb1 123.3(4) . . ? S2A S2 Pb1 113.91(17) 1_565 . ? Pb4 S2 Pb1 130.14(10) 4_576 . ? Pb4 S2 Pb1 60.34(5) 2 . ? Pb3 S2 Pb1 158.03(10) 4_576 . ? Pb1 S2 Pb1 135.66(9) 4_576 . ? O4 S2 Pb3 82.3(5) . 3_666 ? O5 S2 Pb3 103.3(4) . 3_666 ? O6 S2 Pb3 36.9(4) . 3_666 ? S2A S2 Pb3 141.99(18) 1_565 3_666 ? Pb4 S2 Pb3 127.62(10) 4_576 3_666 ? Pb4 S2 Pb3 145.08(9) 2 3_666 ? Pb3 S2 Pb3 85.27(7) 4_576 3_666 ? Pb1 S2 Pb3 62.06(5) 4_576 3_666 ? Pb1 S2 Pb3 88.73(6) . 3_666 ? S1 O1 OH8 121.4(6) . . ? S1 O1 Pb3 143.8(6) . 2_655 ? OH8 O1 Pb3 92.9(3) . 2_655 ? S1 O1 Pb2 83.8(5) . 4_575 ? OH8 O1 Pb2 150.2(5) . 4_575 ? Pb3 O1 Pb2 67.8(2) 2_655 4_575 ? S1 O1 Pb4 74.2(4) . 2_655 ? OH8 O1 Pb4 134.6(5) . 2_655 ? Pb3 O1 Pb4 73.2(2) 2_655 2_655 ? Pb2 O1 Pb4 63.25(16) 4_575 2_655 ? S1 O1 Pb3 103.4(4) . . ? OH8 O1 Pb3 38.5(2) . . ? Pb3 O1 Pb3 111.3(3) 2_655 . ? Pb2 O1 Pb3 126.3(4) 4_575 . ? Pb4 O1 Pb3 170.2(4) 2_655 . ? S1 O1 Pb2 75.0(5) . . ? OH8 O1 Pb2 71.5(3) . . ? Pb3 O1 Pb2 109.5(3) 2_655 . ? Pb2 O1 Pb2 135.2(3) 4_575 . ? Pb4 O1 Pb2 73.1(2) 2_655 . ? Pb3 O1 Pb2 97.1(2) . . ? S1 O2 Pb4 114.8(5) . 1_655 ? S1 O2 Pb2 124.0(6) . 4_575 ? Pb4 O2 Pb2 112.4(3) 1_655 4_575 ? S1 O2 Pb1 98.8(5) . 1_655 ? Pb4 O2 Pb1 84.2(3) 1_655 1_655 ? Pb2 O2 Pb1 114.4(3) 4_575 1_655 ? S1 O2 Pb4 77.4(4) . 2_655 ? Pb4 O2 Pb4 154.1(4) 1_655 2_655 ? Pb2 O2 Pb4 73.0(2) 4_575 2_655 ? Pb1 O2 Pb4 71.1(2) 1_655 2_655 ? S1 O3 Pb4 106.7(6) . 2_655 ? S1 O3 Pb1 98.4(6) . 1_655 ? Pb4 O3 Pb1 82.8(3) 2_655 1_655 ? S1 O3 Pb2 119.6(6) . . ? Pb4 O3 Pb2 103.8(4) 2_655 . ? Pb1 O3 Pb2 136.4(4) 1_655 . ? S1 O3 Pb2 85.2(5) . 3_766 ? Pb4 O3 Pb2 144.3(4) 2_655 3_766 ? Pb1 O3 Pb2 62.0(2) 1_655 3_766 ? Pb2 O3 Pb2 98.5(3) . 3_766 ? S1 S1A Pb2 104.58(19) . 3_766 ? S1 S1A Pb4 80.81(16) . 1_655 ? Pb2 S1A Pb4 75.10(8) 3_766 1_655 ? S1 S1A Pb3 101.76(17) . . ? Pb2 S1A Pb3 151.93(13) 3_766 . ? Pb4 S1A Pb3 119.02(13) 1_655 . ? S1 S1A Pb1 139.9(2) . 2_645 ? Pb2 S1A Pb1 93.53(9) 3_766 2_645 ? Pb4 S1A Pb1 69.53(8) 1_655 2_645 ? Pb3 S1A Pb1 71.88(8) . 2_645 ? S1 S1A Pb1 51.46(13) . 1_655 ? Pb2 S1A Pb1 55.36(6) 3_766 1_655 ? Pb4 S1A Pb1 57.30(6) 1_655 1_655 ? Pb3 S1A Pb1 152.53(11) . 1_655 ? Pb1 S1A Pb1 122.73(10) 2_645 1_655 ? S1 S1A Pb2 63.53(14) . . ? Pb2 S1A Pb2 87.57(9) 3_766 . ? Pb4 S1A Pb2 134.92(11) 1_655 . ? Pb3 S1A Pb2 95.64(8) . . ? Pb1 S1A Pb2 154.33(11) 2_645 . ? Pb1 S1A Pb2 78.49(7) 1_655 . ? S2 O4 Pb1 152.3(7) . . ? S2 O4 OH9 104.5(6) . . ? Pb1 O4 OH9 92.5(3) . . ? S2 O4 OH10 121.3(7) . . ? Pb1 O4 OH10 46.7(2) . . ? OH9 O4 OH10 66.3(3) . . ? S2 O4 Pb4 84.2(5) . 2 ? Pb1 O4 Pb4 76.5(3) . 2 ? OH9 O4 Pb4 168.3(4) . 2 ? OH10 O4 Pb4 102.6(4) . 2 ? S2 O5 Pb4 105.9(5) . 4_576 ? S2 O5 Pb4 89.5(5) . 2 ? Pb4 O5 Pb4 86.9(3) 4_576 2 ? S2 O5 Pb2 153.0(6) . 1_455 ? Pb4 O5 Pb2 101.1(3) 4_576 1_455 ? Pb4 O5 Pb2 89.6(3) 2 1_455 ? S2 O5 Pb1 93.5(5) . 4_576 ? Pb4 O5 Pb1 79.0(3) 4_576 4_576 ? Pb4 O5 Pb1 165.9(3) 2 4_576 ? Pb2 O5 Pb1 93.9(3) 1_455 4_576 ? S2 O6 Pb3 109.1(5) . 4_576 ? S2 O6 Pb1 111.6(5) . 4_576 ? Pb3 O6 Pb1 75.9(2) 4_576 4_576 ? S2 O6 OH9 96.6(5) . . ? Pb3 O6 OH9 136.0(4) 4_576 . ? Pb1 O6 OH9 127.1(4) 4_576 . ? S2 O6 Pb3 127.1(5) . 3_666 ? Pb3 O6 Pb3 123.7(3) 4_576 3_666 ? Pb1 O6 Pb3 85.1(3) 4_576 3_666 ? OH9 O6 Pb3 43.2(2) . 3_666 ? S2 O6 Pb4 55.0(3) . 4_576 ? Pb3 O6 Pb4 69.05(19) 4_576 4_576 ? Pb1 O6 Pb4 66.5(2) 4_576 4_576 ? OH9 O6 Pb4 150.4(4) . 4_576 ? Pb3 O6 Pb4 145.8(3) 3_666 4_576 ? S2 S2A Pb4 81.89(16) 1_545 4_566 ? S2 S2A Pb3 84.78(16) 1_545 4_566 ? Pb4 S2A Pb3 79.49(10) 4_566 4_566 ? S2 S2A Pb2 158.9(2) 1_545 3_666 ? Pb4 S2A Pb2 97.65(11) 4_566 3_666 ? Pb3 S2A Pb2 115.98(12) 4_566 3_666 ? S2 S2A Pb4 76.16(15) 1_545 2_545 ? Pb4 S2A Pb4 78.87(10) 4_566 2_545 ? Pb3 S2A Pb4 152.88(13) 4_566 2_545 ? Pb2 S2A Pb4 83.05(9) 3_666 2_545 ? Pb4 O7 Pb1 112.2(3) . . ? Pb4 O7 Pb3 117.3(4) . . ? Pb1 O7 Pb3 101.2(3) . . ? Pb4 O7 Pb2 116.0(3) . 3_666 ? Pb1 O7 Pb2 104.6(3) . 3_666 ? Pb3 O7 Pb2 103.7(3) . 3_666 ? Zn OH8 Pb1 103.3(4) . . ? Zn OH8 Pb3 102.2(4) . . ? Pb1 OH8 Pb3 98.9(3) . . ? Zn OH8 O1 126.7(5) . . ? Pb1 OH8 O1 122.0(4) . . ? Pb3 OH8 O1 97.4(4) . . ? Zn OH8 O6 163.1(5) . 4_575 ? Pb1 OH8 O6 67.6(3) . 4_575 ? Pb3 OH8 O6 66.6(3) . 4_575 ? O1 OH8 O6 69.0(4) . 4_575 ? Zn OH8 Pb3 140.2(4) . 2_655 ? Pb1 OH8 Pb3 79.7(2) . 2_655 ? Pb3 OH8 Pb3 116.6(3) . 2_655 ? O1 OH8 Pb3 43.6(2) . 2_655 ? O6 OH8 Pb3 54.4(2) 4_575 2_655 ? Zn OH8 Pb2 61.7(2) . 3_666 ? Pb1 OH8 Pb2 64.6(2) . 3_666 ? Pb3 OH8 Pb2 64.0(2) . 3_666 ? O1 OH8 Pb2 161.3(4) . 3_666 ? O6 OH8 Pb2 101.4(3) 4_575 3_666 ? Pb3 OH8 Pb2 143.3(2) 2_655 3_666 ? Zn OH9 Pb3 101.5(4) . 3_666 ? Zn OH9 Pb2 103.7(4) . . ? Pb3 OH9 Pb2 102.2(3) 3_666 . ? Zn OH9 O4 93.7(4) . . ? Pb3 OH9 O4 109.0(4) 3_666 . ? Pb2 OH9 O4 140.3(4) . . ? Zn OH9 O6 127.1(4) . . ? Pb3 OH9 O6 70.8(3) 3_666 . ? Pb2 OH9 O6 129.2(4) . . ? O4 OH9 O6 46.8(3) . . ? Zn OH9 Pb1 61.0(2) . 3_666 ? Pb3 OH9 Pb1 64.8(2) 3_666 3_666 ? Pb2 OH9 Pb1 66.8(2) . 3_666 ? O4 OH9 Pb1 149.9(4) . 3_666 ? O6 OH9 Pb1 135.3(3) . 3_666 ? Zn OH10 Pb1 100.3(3) . . ? Zn OH10 Pb2 103.4(3) . 3_666 ? Pb1 OH10 Pb2 103.8(4) . 3_666 ? Zn OH10 O4 92.1(3) . . ? Pb1 OH10 O4 61.0(3) . . ? Pb2 OH10 O4 160.4(4) 3_666 . ? Zn OH10 O3 161.4(4) . 1_455 ? Pb1 OH10 O3 63.5(3) . 1_455 ? Pb2 OH10 O3 89.9(3) 3_666 1_455 ? O4 OH10 O3 72.5(4) . 1_455 ? Zn OH10 Pb3 61.8(2) . . ? Pb1 OH10 Pb3 64.6(2) . . ? Pb2 OH10 Pb3 66.2(2) 3_666 . ? O4 OH10 Pb3 112.6(3) . . ? O3 OH10 Pb3 114.0(3) 1_455 . ? _refine_diff_density_max 2.124 _refine_diff_density_min -1.746 _refine_diff_density_rms 0.440 _shelx_res_file ; TITL Redmond-3 redmond3.res created by SHELXL-2016/6 at 22:17:50 on 05-Jul-2021 CELL 0.71075 9.16723 10.65760 14.06200 90.00000 101.17300 90.00000 ZERR 2 0.00040 0.00035 0.00099 0.00000 0.00710 0.00000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC H O PB S ZN UNIT 12 40 16 16 2 L.S. 5 omit 0 2 3 omit 0 2 1 CONN 15 3.0 PB1 CONN 15 3.0 PB2 CONN 15 3.0 PB3 CONN 15 3.0 PB4 EQIV $1 x, 1.5-y, -0.5+z EQIV $2 -1+x, y, z BIND OH8 O1 BIND OH8 O6_$1 BIND OH9 O4 BIND OH9 O6 BIND OH10 O3_$2 BIND OH10 O4 FMAP 2 PLAN 20 ACTA SIZE 0.110 0.100 0.090 WGHT 0.030300 7.426800 EXTI 0.000613 FVAR 0.13357 PB1 3 0.243908 0.657419 0.330748 11.00000 0.01398 0.01327 = 0.01753 0.00240 -0.00336 0.00145 PB2 3 0.840767 0.659863 0.587830 11.00000 0.01751 0.01628 = 0.01358 0.00182 0.00032 -0.00257 PB3 3 0.442815 0.390149 0.262321 11.00000 0.01378 0.02327 = 0.01684 -0.00532 0.00248 0.00067 PB4 3 0.020647 0.438401 0.140315 11.00000 0.01548 0.01909 = 0.01332 0.00026 -0.00310 -0.00432 ZN 5 0.500000 0.500000 0.500000 10.50000 0.01582 0.01936 = 0.00894 0.00222 -0.00434 0.00103 S1 4 0.854200 0.617045 0.305062 11.00000 0.01067 0.01351 = 0.01546 0.00002 0.00246 -0.00060 S2 4 0.273743 0.886869 0.569985 11.00000 0.01703 0.01398 = 0.01105 -0.00227 -0.00299 0.00366 O1 2 0.707790 0.674136 0.288544 11.00000 0.01286 0.01458 = 0.08600 0.00727 0.01813 0.01030 O2 2 0.926357 0.642934 0.222895 11.00000 0.03346 0.02284 = 0.02466 -0.00300 0.01090 0.00164 O3 2 0.949322 0.669917 0.394313 11.00000 0.04094 0.04738 = 0.02719 -0.01156 -0.00560 -0.01063 S1A 4 0.835283 0.431298 0.318131 11.00000 0.02592 0.01635 = 0.03323 0.00015 0.00865 0.00418 O4 2 0.312525 0.817807 0.489779 11.00000 0.04243 0.03640 = 0.03282 -0.01395 0.00368 0.00960 O5 2 0.126912 0.856096 0.587877 11.00000 0.02243 0.02677 = 0.03267 0.00227 0.00474 0.00516 O6 2 0.386147 0.868356 0.661481 11.00000 0.03005 0.01757 = 0.02438 -0.00758 -0.00978 0.01024 S2A 4 0.262337 0.073020 0.537935 11.00000 0.03219 0.01937 = 0.02179 0.00309 0.00494 0.00174 O7 2 0.202597 0.451536 0.276355 11.00000 0.00695 0.00993 = 0.01050 -0.00051 0.00066 0.00080 OH8 2 0.484005 0.574565 0.364331 11.00000 0.01524 0.01423 = 0.00920 0.00359 -0.00355 0.00461 OH9 2 0.578375 0.666353 0.579000 11.00000 0.01480 0.02230 = 0.01171 0.00185 -0.00250 0.00567 OH10 2 0.264100 0.536449 0.470008 11.00000 0.00966 0.00676 = 0.02169 0.00411 0.00053 -0.00533 HKLF 4 REM Redmond-3 REM R1 = 0.0346 for 2061 Fo > 4sig(Fo) and 0.0420 for all 2372 data REM 170 parameters refined using 0 restraints END WGHT 0.0303 7.4271 REM Highest difference peak 2.124, deepest hole -1.746, 1-sigma level 0.440 Q1 1 0.3569 0.3198 0.2435 11.00000 0.05 2.12 Q2 1 0.9432 0.7459 0.5968 11.00000 0.05 1.91 Q3 1 0.7971 0.5832 0.6194 11.00000 0.05 1.85 Q4 1 0.0283 0.9474 0.5934 11.00000 0.05 1.80 Q5 1 0.5211 0.3411 0.2183 11.00000 0.05 1.77 Q6 1 0.5057 0.2604 0.2312 11.00000 0.05 1.76 Q7 1 0.9003 0.5895 0.5828 11.00000 0.05 1.69 Q8 1 -0.0741 0.3855 0.1854 11.00000 0.05 1.62 Q9 1 0.8734 0.5692 0.5590 11.00000 0.05 1.57 Q10 1 0.1466 0.1106 0.5770 11.00000 0.05 1.56 Q11 1 0.9429 0.6129 0.5338 11.00000 0.05 1.54 Q12 1 0.3867 0.5046 0.2798 11.00000 0.05 1.54 Q13 1 -0.0460 0.3606 0.1226 11.00000 0.05 1.54 Q14 1 0.1138 0.5300 0.1568 11.00000 0.05 1.53 Q15 1 0.1574 0.7980 0.4164 11.00000 0.05 1.51 Q16 1 0.2497 0.5296 0.2834 11.00000 0.05 1.49 Q17 1 0.1542 0.7311 0.3091 11.00000 0.05 1.49 Q18 1 0.1243 0.4846 0.0993 11.00000 0.05 1.48 Q19 1 0.7125 0.7082 0.5137 11.00000 0.05 1.43 Q20 1 0.7390 0.7248 0.5437 11.00000 0.05 1.43 ; _shelx_res_checksum 39729 _shelx_hkl_file ; 1 1 -1 3603.04 113.52 -1 -1 1 4058.29 121.21 1 -1 -1 3117.41 95.15 -1 -1 1 3789.77 122.69 -1 1 1 3094.15 96.51 -1 0 2 424.80 10.67 1 0 -2 428.81 10.98 -1 -1 -1 357.38 12.56 1 1 1 448.20 10.13 1 -1 1 409.33 11.68 1 1 1 334.53 10.04 -1 -1 -1 432.60 9.75 -1 1 -1 447.14 12.42 0 -1 -2 30.49 2.29 0 1 2 30.91 1.76 0 -2 0 387.61 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-5 8 75.26 13.17 -4 5 8 106.05 10.87 4 5 -8 95.58 18.76 4 -5 -8 84.35 10.20 3 5 7 204.16 22.77 3 5 7 208.82 18.26 -3 -5 -7 209.69 20.39 3 -5 7 154.23 31.92 2 -5 8 1605.20 131.61 2 5 8 2579.60 114.83 2 5 8 2484.15 123.43 -2 -5 -8 1897.36 90.02 6 -5 -3 447.46 37.61 6 5 -3 433.96 40.75 6 5 -3 498.59 44.75 -6 5 3 446.73 37.17 -6 -5 3 455.25 45.74 3 2 9 1439.47 66.64 -3 -2 -9 1487.31 96.50 3 -2 9 1235.89 99.52 3 2 9 1468.60 88.03 -5 4 -5 638.30 91.13 5 4 5 681.76 44.07 5 -4 5 553.54 56.46 5 4 5 655.78 46.91 -5 -4 -5 541.54 46.27 -5 -4 8 10.06 12.04 -5 4 8 14.75 7.85 5 -4 -8 15.88 7.48 5 4 -8 16.11 9.84 5 4 -8 25.60 13.27 -7 -3 2 434.54 49.14 -7 3 2 416.17 41.96 7 -3 -2 457.26 44.31 7 3 -2 346.26 40.59 7 3 -2 447.23 56.84 6 4 -6 243.76 40.23 -6 4 6 283.69 38.74 -6 -4 6 248.02 32.12 6 4 -6 203.87 31.56 6 -4 -6 203.45 22.70 7 2 -5 267.53 34.80 7 -2 -5 256.79 31.24 -7 2 5 314.87 36.60 -7 -2 5 270.01 40.31 7 2 -5 316.70 29.33 -4 -7 4 695.20 54.21 4 7 -4 960.34 78.64 4 7 -4 933.08 65.97 -4 7 4 996.58 54.01 -4 -7 4 769.13 55.18 4 -7 -4 740.08 43.31 -3 -4 -8 598.86 42.21 3 4 8 577.63 38.29 3 -4 8 365.93 56.41 3 4 8 609.98 34.56 -7 0 6 2392.90 153.41 7 0 -6 2215.68 137.26 3 7 4 384.48 58.06 -3 -7 -4 319.04 20.39 3 7 4 377.45 17.87 3 -7 4 242.11 35.26 -3 -7 -4 269.50 27.93 6 -5 0 983.82 78.31 6 5 0 1002.72 63.61 6 5 0 1209.03 75.83 -6 -5 0 1050.55 77.62 -6 5 0 1037.80 71.73 0 -4 10 82.52 26.15 0 4 10 106.69 12.35 0 4 10 124.53 12.80 0 -4 10 104.92 30.93 0 -4 10 108.28 12.51 -6 2 8 248.01 27.76 -6 -2 8 217.50 46.06 6 2 -8 190.73 21.33 6 -2 -8 276.88 26.88 6 2 -8 189.92 31.22 7 -3 -3 62.91 17.22 7 3 -3 63.00 15.08 -7 -3 3 54.88 20.14 7 3 -3 37.65 17.49 -7 3 3 82.43 27.10 -2 -6 -7 26.04 6.37 2 6 7 24.74 5.20 -2 -6 -7 8.45 7.48 2 -6 7 -0.47 14.01 -7 2 -1 415.87 46.50 7 2 1 501.75 48.88 7 -2 1 507.58 52.41 7 2 1 494.30 40.62 -7 -2 -1 421.67 48.22 -7 3 1 871.71 68.25 7 -3 -1 1028.39 76.13 7 3 -1 975.79 64.68 -7 -3 1 999.10 80.12 7 3 -1 835.93 66.66 -4 2 -8 116.08 27.81 4 -2 8 105.72 24.50 4 2 8 99.40 11.82 -4 -2 -8 100.78 22.17 4 2 8 100.46 19.91 6 0 5 18.43 14.22 -6 0 -5 6.96 12.73 -7 0 -2 914.67 107.64 7 0 2 1045.74 85.46 3 -8 -1 162.54 15.74 3 8 -1 197.84 20.66 -3 -8 1 121.08 25.22 -3 -8 1 174.68 18.17 0 -2 11 56.81 29.90 0 -2 11 25.91 17.02 0 2 11 39.37 12.04 0 2 11 45.15 19.55 0 -2 11 38.94 5.24 -5 3 -6 660.75 99.09 -5 -3 -6 663.11 52.68 5 3 6 669.18 39.99 5 -3 6 570.63 61.50 5 3 6 693.46 54.49 -2 -8 4 1264.86 75.15 -2 -8 4 1007.36 83.37 2 -4 9 450.73 62.60 2 4 9 697.80 35.43 2 4 9 776.23 41.88 -1 -8 -4 6.70 10.06 1 -8 4 6.54 10.72 1 -8 4 17.60 9.94 2 2 10 43.48 14.46 2 2 10 66.48 8.94 2 -2 10 46.71 19.61 7 1 -6 7.64 8.99 7 1 -6 17.13 11.39 -7 1 6 24.60 11.74 7 -1 -6 3.63 11.22 -7 -1 6 17.03 13.46 -3 -5 9 250.01 36.77 -3 5 9 442.21 19.39 -3 -5 9 340.40 23.69 -5 3 9 233.12 22.16 -5 -3 9 203.37 28.77 5 3 -9 216.25 35.98 5 -3 -9 191.85 22.38 5 3 -9 204.49 20.80 -3 -6 -6 25.49 10.53 -3 -6 -6 44.68 8.63 3 -6 6 9.54 17.02 3 6 6 42.91 14.49 3 6 6 53.66 8.17 -6 5 4 32.23 11.61 6 5 -4 54.08 13.96 6 5 -4 39.83 14.77 -6 -5 4 33.64 15.39 6 -5 -4 15.39 17.84 -3 -8 0 574.84 53.28 3 -8 0 677.71 57.31 -3 -8 0 693.35 57.12 3 8 0 841.98 45.66 -4 -7 -2 22.65 11.69 -4 -7 -2 28.51 10.36 4 7 2 46.59 15.96 4 7 2 25.38 8.30 4 -7 2 25.58 12.17 -3 -7 6 1375.76 90.36 -3 -7 6 1599.91 100.41 5 5 4 1469.64 86.27 5 -5 4 1244.65 133.06 5 5 4 1376.74 78.87 -5 5 -4 1371.08 104.39 -5 -5 -4 1225.58 77.63 5 0 7 -7.42 10.36 -5 0 -7 3.07 16.62 3 -8 -2 6.57 5.23 -3 -8 2 0.17 11.08 3 8 -2 11.98 8.33 -3 -8 2 14.79 10.09 5 5 -7 234.61 35.41 5 -5 -7 224.54 18.16 -5 -5 7 236.89 32.08 -5 -5 7 227.17 22.70 -5 5 7 246.13 20.38 5 5 -7 294.23 30.27 -4 -3 10 13.15 10.38 -4 3 10 9.93 6.71 4 3 -10 9.70 7.30 4 -3 -10 8.43 8.01 -5 -6 -2 123.41 21.49 -5 6 -2 158.03 39.67 5 6 2 162.27 18.34 -5 -6 -2 123.21 22.33 5 -6 2 148.67 39.00 5 6 2 215.60 27.21 -5 0 10 358.51 34.45 5 0 -10 362.05 40.85 5 0 -10 315.66 19.10 -2 -8 -3 0.81 9.03 2 -8 3 2.07 8.59 -2 -8 -3 2.71 4.12 2 8 3 19.26 5.94 6 1 5 1943.69 101.01 -6 1 -5 1854.26 132.37 6 -1 5 1796.13 141.11 6 1 5 1948.82 140.67 -6 -1 -5 1793.75 124.94 -3 -2 11 233.65 48.96 -3 2 11 339.54 25.73 -5 -6 5 399.61 34.53 5 6 -5 481.61 66.87 -5 6 5 403.32 26.59 5 6 -5 467.70 43.29 -5 -6 5 469.38 41.12 5 -6 -5 385.10 25.55 1 -7 -7 52.25 15.31 -1 -7 7 48.08 16.12 -1 -7 7 70.66 18.32 7 -1 2 846.50 74.62 -7 1 -2 761.95 67.77 -7 -1 -2 590.30 74.35 7 1 2 898.13 73.45 7 -3 -4 4.82 7.23 -7 3 4 8.96 7.55 7 3 -4 -10.92 6.71 7 3 -4 5.92 7.95 -7 -3 4 1.28 9.16 4 -5 6 604.70 65.10 4 5 6 890.71 52.64 4 5 6 847.00 48.16 -4 -5 -6 803.92 50.01 1 0 11 11.53 11.41 -6 3 -4 1374.40 137.79 6 -3 4 1346.12 145.89 6 3 4 1426.98 106.71 6 3 4 1574.07 98.42 -6 -3 -4 1282.32 93.11 4 4 7 710.55 48.86 4 4 7 714.38 41.87 4 -4 7 517.01 60.63 -4 -4 -7 726.29 49.23 -3 -4 10 552.72 80.09 -3 4 10 860.65 46.94 -3 -4 10 752.48 44.50 -5 -1 -7 374.40 42.60 -5 1 -7 391.36 48.32 5 1 7 351.87 25.55 5 1 7 362.24 40.23 5 -1 7 328.76 47.24 -4 6 7 331.10 16.57 -4 -6 7 281.74 26.56 4 6 -7 344.60 60.53 4 6 -7 259.82 40.54 -4 -6 7 302.76 32.59 4 -6 -7 271.35 15.61 7 3 0 960.87 72.68 7 -3 0 1071.08 82.21 7 3 0 1003.68 66.00 -7 -3 0 1006.20 82.20 -7 3 0 831.70 71.45 1 -5 9 34.16 17.21 -1 -5 -9 18.64 5.57 1 5 9 23.61 6.22 5 -1 -10 469.49 64.63 -5 1 10 477.08 37.74 5 -1 -10 377.17 21.35 5 1 -10 423.67 25.32 5 1 -10 493.27 50.29 -5 -1 10 486.29 60.65 0 -7 7 232.26 40.60 0 -7 -7 223.26 24.38 0 -7 7 231.25 32.31 0 -7 7 267.41 36.28 -6 5 -1 265.29 33.05 -6 -5 -1 283.07 51.49 6 -5 1 217.15 36.84 6 5 1 291.13 40.59 6 5 1 298.99 33.21 -3 -8 -1 352.11 25.37 -3 -8 -1 328.90 34.78 3 -8 1 325.45 31.56 3 8 1 470.38 53.40 3 8 1 450.22 25.39 6 -4 3 283.20 40.16 -6 -4 -3 246.35 34.00 6 4 3 287.81 31.75 6 4 3 280.68 29.35 -6 4 -3 262.71 58.81 -3 -6 8 132.24 17.77 -3 6 8 166.20 7.16 -3 -6 8 144.57 25.03 1 6 8 6.22 2.88 1 -6 8 4.50 12.45 -1 -6 -8 4.21 5.07 1 -1 11 345.30 62.24 1 1 11 315.26 34.57 -1 -8 5 219.22 27.35 -1 -8 5 210.26 32.43 1 -8 -5 185.68 32.35 -1 3 11 2255.12 117.82 -1 -3 11 1824.95 133.23 -1 3 11 2034.32 98.58 -1 -3 11 1953.96 70.36 -3 -8 3 1576.30 108.93 -3 -8 3 1942.47 131.01 3 -8 -3 1746.68 70.05 2 -7 -7 466.76 44.13 -2 -7 7 375.18 56.10 -2 -7 7 478.75 45.11 0 -8 -5 94.20 21.99 0 -8 5 127.21 28.08 0 -8 5 145.25 26.25 0 -8 5 131.33 33.91 -2 3 11 1471.30 66.68 -2 -3 11 1490.56 50.84 -2 -3 11 1088.97 88.36 -4 0 11 -2.03 6.65 4 0 -11 2.07 2.66 -4 7 5 296.78 15.18 4 7 -5 283.79 34.03 -4 -7 5 240.36 43.10 -4 -7 5 209.72 26.84 4 7 -5 281.15 42.55 4 -7 -5 225.59 17.96 7 2 -6 10.70 9.16 7 -2 -6 5.14 10.32 7 2 -6 13.06 11.89 -7 -2 6 20.34 13.19 -7 2 6 11.56 12.13 3 -3 9 1.80 13.60 -3 -3 -9 8.64 11.02 3 3 9 19.89 9.72 3 3 9 16.28 9.21 6 0 -9 17.39 6.28 6 0 -9 2.12 11.11 -6 0 9 -2.00 10.06 -6 5 5 939.18 55.44 6 5 -5 932.26 66.71 6 -5 -5 695.49 49.19 -6 -5 5 927.00 102.12 6 5 -5 799.37 66.31 -4 -1 11 10.30 16.26 4 1 -11 14.98 5.14 4 -1 -11 12.31 3.21 -4 1 11 4.65 14.21 6 -2 5 824.78 78.04 -6 2 -5 1029.19 109.00 -6 -2 -5 753.47 68.28 6 2 5 849.46 51.96 6 2 5 963.19 76.63 -7 2 -2 409.07 50.54 -7 -2 -2 415.32 49.26 7 2 2 550.14 41.85 7 -2 2 479.89 57.57 7 2 2 473.56 53.65 7 3 -5 1650.26 96.26 -7 3 5 1751.38 111.40 7 3 -5 1427.58 104.19 7 -3 -5 1398.46 95.82 -7 -3 5 1745.85 120.98 -2 -7 -6 995.93 37.91 -2 -7 -6 797.38 71.59 2 7 6 1110.91 38.88 2 -7 6 721.62 72.88 4 6 5 618.46 35.56 4 -6 5 555.56 81.03 -4 -6 -5 572.06 52.19 -4 -6 -5 522.14 40.27 4 6 5 716.88 51.30 1 -4 10 131.93 31.78 1 4 10 145.05 15.42 7 0 -7 12.99 8.15 -7 0 7 7.87 12.12 7 0 -7 9.78 11.04 6 3 -8 0.35 8.11 -6 -3 8 -9.70 7.73 -6 3 8 1.51 9.22 6 3 -8 3.74 5.50 6 -3 -8 1.36 5.60 6 -1 -9 26.08 11.51 -6 1 9 26.24 11.81 6 -1 -9 0.54 7.40 6 1 -9 40.15 13.54 6 1 -9 21.18 7.87 -6 -1 9 27.56 19.68 5 2 7 9.89 11.02 5 -2 7 -0.68 12.70 -5 2 -7 0.83 13.70 -5 -2 -7 3.16 11.00 5 2 7 12.92 6.63 7 3 1 41.74 27.01 -7 3 -1 33.21 16.77 7 3 1 47.53 14.45 7 -3 1 42.85 19.75 -7 -3 -1 32.73 17.72 6 4 -7 197.22 24.72 -6 4 7 215.04 24.09 -6 -4 7 158.24 29.18 6 4 -7 178.95 32.33 6 -4 -7 163.66 19.56 -2 -8 5 2259.90 133.29 -2 -8 5 2009.89 138.76 0 -9 0 2.26 10.61 4 3 8 217.57 30.19 4 -3 8 197.65 37.10 4 3 8 251.18 20.36 -4 -3 -8 276.53 31.61 -5 2 10 117.40 28.98 5 2 -10 135.10 22.37 5 2 -10 141.44 29.17 -5 -2 10 110.52 23.66 5 -2 -10 116.78 33.68 4 7 3 1892.53 84.63 4 7 3 2203.79 133.26 4 -7 3 1583.12 111.80 -4 -7 -3 1630.81 88.81 -4 -7 -3 1434.11 94.03 3 8 2 401.48 22.04 -3 -8 -2 290.63 24.03 -3 -8 -2 303.38 31.93 3 -8 2 324.13 45.51 3 8 2 404.29 51.71 0 3 11 338.40 36.93 0 -3 11 273.57 38.93 0 3 11 239.49 24.03 0 -3 11 244.39 45.30 0 -3 11 235.29 15.26 2 3 10 64.57 14.12 2 3 10 67.66 12.93 2 -3 10 38.74 21.46 1 2 11 1.42 9.75 1 -2 11 -0.27 9.23 0 -9 -1 122.18 32.64 0 -9 -1 183.41 19.67 0 -9 1 174.94 19.78 0 -9 -1 154.01 10.59 0 -9 1 136.85 51.95 0 -9 1 163.77 14.77 7 0 3 14.76 13.54 -7 0 -3 -1.15 20.14 7 1 -7 -6.12 6.47 7 1 -7 -10.89 9.00 -7 1 7 1.18 8.82 -7 -1 7 -4.29 10.13 7 -1 -7 8.43 7.93 5 -6 3 78.64 21.03 -5 -6 -3 67.56 16.99 -5 -6 -3 39.76 16.14 5 6 3 75.00 22.16 5 6 3 124.30 20.49 -5 6 -3 97.82 22.91 -3 -7 -5 975.54 44.07 3 -7 5 752.46 70.93 3 7 5 1089.39 79.66 3 7 5 1089.94 41.56 -3 -7 -5 766.39 54.74 -3 -8 4 82.57 17.44 3 -8 -4 82.87 4.66 -3 -8 4 58.98 20.03 5 6 -6 40.49 19.59 5 6 -6 66.52 19.28 5 -6 -6 59.23 8.86 -5 6 6 60.20 9.85 -5 -6 6 40.80 17.02 -5 -6 6 44.80 13.62 2 8 4 1556.97 47.83 -2 -8 -4 1026.01 74.42 2 -8 4 876.17 76.25 -2 -8 -4 1252.22 44.40 1 -8 5 1892.13 136.51 1 -8 5 2215.66 137.50 -1 -8 -5 1819.68 114.97 -1 -7 -7 430.51 34.13 1 -7 7 469.02 83.08 -3 -3 11 869.43 76.88 -3 3 11 1315.82 76.66 3 -3 -11 1064.56 41.75 6 5 2 954.17 64.18 -6 5 -2 1008.37 79.03 -6 -5 -2 953.84 72.56 6 5 2 1131.86 74.75 6 -5 2 1024.01 83.07 7 -4 -2 28.01 14.62 -7 4 2 6.40 21.06 7 4 -2 33.16 14.04 7 4 -2 26.43 13.67 -7 -4 2 29.77 25.74 -1 -9 0 64.09 21.33 1 -9 0 67.19 9.28 1 -9 0 65.15 25.90 1 -9 0 65.85 15.67 -1 -9 0 53.63 8.83 -1 5 10 807.16 27.92 1 -5 -10 550.59 25.88 -1 -5 10 573.92 35.78 -1 5 10 807.72 40.88 -1 -5 10 612.15 88.85 -1 6 9 475.04 10.20 -1 -6 9 429.21 48.87 1 -6 -9 429.68 27.07 -1 -6 9 435.45 35.43 -1 6 9 516.56 11.74 7 1 3 35.02 14.07 -7 -1 -3 56.68 18.34 7 -1 3 25.55 21.42 7 1 3 50.43 20.54 -7 1 -3 48.27 18.85 1 -9 -1 415.27 57.23 1 -9 -1 391.75 26.05 1 -9 -1 416.41 22.08 -1 -9 1 407.23 48.66 -1 -9 1 407.86 25.49 -7 -4 3 545.50 53.79 -7 4 3 492.61 43.54 7 4 -3 431.84 43.67 7 4 -3 400.58 44.31 7 -4 -3 492.80 44.43 7 4 -1 362.46 39.33 7 4 -1 367.25 39.86 -7 -4 1 381.51 71.93 -7 4 1 390.07 41.11 7 -4 -1 406.77 42.80 -5 7 1 211.12 25.86 -5 -7 1 193.83 27.29 5 7 -1 272.21 54.71 5 7 -1 206.97 23.29 -5 -7 1 173.21 27.42 5 -7 -1 228.46 25.84 5 -7 -2 239.43 24.02 -5 7 2 224.13 23.31 5 7 -2 317.19 40.20 -5 -7 2 231.34 29.72 5 7 -2 226.98 25.69 -5 -7 2 190.75 28.47 3 0 10 86.29 20.34 3 0 10 69.20 8.01 4 5 -9 776.58 61.28 -4 -5 9 713.88 41.60 -4 5 9 904.84 52.95 -4 -5 9 673.15 60.87 4 -5 -9 736.97 40.14 -2 0 12 1297.16 85.56 -4 2 11 947.50 53.85 4 -2 -11 679.44 25.26 4 2 -11 847.94 41.79 -4 -2 11 722.07 61.42 -1 0 12 282.62 53.42 -1 0 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27.19 -10 4 7 726.25 125.51 1 1 16 0.40 29.77 1 -1 16 178.37 33.35 1 1 16 1.44 29.23 1 -1 16 124.05 33.91 7 -6 -12 -3.03 16.21 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 61519